Elastic recoil detection analysis on the ANSTO heavy ion microprobe

The heavy ion microprobe at the Australian Nuclear Science and Technology Organisation is capable of focussing heavy ions with an ME/q² of up to 100 amu MeV. This makes the microprobe ideally suited for heavy ion elastic recoil detection analysis (ERDA). However, beam currents on a microprobe are usually very small, which requires a detection system with a large solid angle. We apply microbeam heavy ion ERDA using a large solid angle ΔE−E telescope with a gas ΔE detector to layered structures. We demonstrate the capability to measure oxygen and carbon with a lateral resolution of 20 μm, together with determination of the depth of the contamination in thin deposited layers.     

Layout of a nuclear microprobe beamline using a liquid metal ion source

The Bochum solenoid lens microprobe will be installed in a new configuration which can be fed both by the 4 MV Dynamitron tandem accelerator and by a new 500 kV accelerator of extremely low energy-spread (ΔE/E 10⁻⁵). Apart from a conventional duoplasmatron ion source, a commercial gallium liquid metal ion source (LMIS) will be implemented in this accelerator. Microprobe optics will benefit from the high brightness of the LMIS ( 10⁵ Am⁻²sr⁻¹eV⁻¹), thus enabling an increased lateral resolution. Ion optical ray tracing, simulating the accelerator tube and the solenoid lens, has allowed one to specify the beam parameters required at the accelerator entrance to yield a micrometer focus at the target position. Using this information and further simulations, the accelerator injection optics can be particularly optimized for the new microbeam line.     

Contribution of uranium diffusion on creep behavior of uranium dicarbide

Compressive creep tests of uranium dicarbide (UC₂) have been conducted. The general equation best describing the creep rate over the temperature range 1200–1400°C and over the stress range 2000–15000 psi is represented by the sum of two exponential terms ge =A(σ/E)^0.9 exp(−39.6 ± 1.0/RT) + B(σ/E)^4.5 exp(−120.6 ± 1.7/RT), where pre-exponential factors are A(σ/E)^0.9 = 12.3/h at low stress region (3000 psi) and B(σ/E)^4.5 = 3.17 × 10¹³/h at high stress region (9000 psi), and the activation energy is given in kcal/mol. Each term of this experimental equation indicates that important processes occurring during the steady state creep are grain-boundary diffusion of the Coble model at low stress region and the Weertman dislocation climb model at high stress region. Both mechanisms are related to migration of uranium vacancies.     

The Stuttgart positron beam, its performance and recent experiments

A monoenergetic MeV positron (e⁺) beam, with a flux at present of 6 × 10⁴ e⁺/s in the energy range of 0.5 to 6.5 MeV, has been installed at the Stuttgart Pelletron accelerator. The stabilization and the absolute calibration of the energy E is monitored by a Ge detector with real-time feedback; a relative energy stability of ΔE/E 10⁻⁴ is obtained. So far, e⁺e⁻ scattering and annihilation-in-flight experiments for investigating the low-energy e⁺e⁻ interaction as well as β⁺ γ positron lifetime measurements in condensed matter have been performed. The advantages of the β⁺ γ method compared to the conventional γγ coincidence technique have been demonstrated. Recently, triple-coincidence positron “age-momentum correlation” measurements have been carried out on fused quartz. A brief account is given on the development of a “positron clock” aiming at a substantial improvement of the time resolution of the β⁺ γ positron lifetime measurements.     

The thermal conductivity of UO2 vapor

The thermal conductivity, λ of a saturated vapor over UO_1.96 is calculated in the temperature range 3000–6000 K. The calculation shows that the contribution to λ from the transport of reaction enthalpy dominates all other contributions. All possible reactions of the gaseous species UO₃, UO₂, UO, U, O, and O₂ are included in the calculation. We fit the total thermal conductivity to the empirical equation λ = exp(a+ b/T+cT+dT² + eT³), with λ in cal/(cm s K), T in kelvins, a = 268.90, B = − 3.1919 × 10⁵, C = −8.9673 × 10⁻², d = 1.2861 × 10⁻⁵, and E = −6.7917 × 10⁻¹⁰.     

Measurement of the H2-D mass difference with a nuclear microprobe

A 1.24 MeV deuteron (D) beam mixed with a H₂ molecular beam was separated with a microslit system of a nuclear microprobe consisting of a 100 μm diameter object and a 1 mm diameter aperture diaphragm. D was distinguished from H₂ by Rutherford backscattering (RBS) on a thin Au film. By slightly changing the magnetic field strength of the beam steerer installed in front of the object diaphragm, the maximum and the minimum RBS D/H₂ ratios were found to be 50.3 and 1.5, respectively. M/ΔM = 3.9 × 10³ was obtained as the mass resolution of the nuclear microprobe. The transmission of this system was 2 × 10⁻³.     

High energy resolution PIXE with high efficiency using the heavy ion microbeam

An X-ray crystal spectrometer using a position sensitive proportional counter combined with tandem microbeam line at Osaka National Research Institute have been developed. This system realizes high energy resolution PIXE analysis using a heavy ion microbeam (E < 6 MeV) with reasonable detection efficiency. The design of the spectrometer, such as detection geometry, detectable energy range and energy resolution, are described. This system was applied to high energy resolution PIXE analysis of Ti, SUS and Si with 2 MeV proton and 5 MeV Si³⁺ focused or collimated beams. The best energy resolution was 2 eV for the Si K line.     

Investigation of in-reactor creep and irradiation growth of zirconium-2.5 wt% niobium channel tubes

We summarize the diametral creep results obtained in the MR reactor of the Kurchatov Institute of Atomic Energy on zirconium-2.5 wt% niobium pressure tubes of the type used in RBMK-1000 power reactors. The experiments that lasted up to 30 000 h cover a temperature range of 270 to 350°C, neutron fluxes between 0.6 and 4.0 ×10¹³ n/cm² · s (E > 1 MeV) and stresses of up to 16 kgf/mm². Diametral strains of up to 4.8% have been measured. In-reactor creep results have been analyzed in terms of thermal and irradiation creep components assuming them to be additive. The thermal creep rate is given by a relationship of the type ε_th = A₁ exp [(A₂ + A _3σt) T] and the irradiation component by ε_rad = A_4σtø(T − A₅), where T = temperature, σ_t = hoop stress, ø = neutron flux and a₁ to A₅ are constants. Irradiation growth experiments carried out at 280° C on specimens machined from pressure tubes showed a non-linear dependence of growth strain on neutron fluence up to neutron fluences of 5 × 10²⁰ n/cm². The significance of these results to the elongation of RBMK reactor pressure tubes is discussed.     

A scanning positron microscope for defect analysis in materials science

The realisation of a scanning positron microscope will be presented and discussed. A positron beam with a variable energy from 0.5 to 30 keV, with a spot diameter of 1 μm or below, can be scanned over an area of 0.6 × 0.6 mm². This beam is formed after a double stage stochastic cooling (moderation) of positrons emitted from a radioactive isotope. In addition the positron beam will be pulsed in order to have a well-defined time base for positron lifetime measurements. In the system included is a conventional scanning electron microprobe for surface analysis. The design of the scanning positron microscope is dominated by the special demands of positron physics.     

Design of a magnetic spectrograph for surface, interface and thin-layer analysis

The design of a magnetic spectrograph of the QDQ type, to be coupled to a 6 MV Van de Graaff accelerator for the analysis with Rutherford backscattering and recoil spectroscopy of surfaces and thin layers, will be shown. Due to the high energy resolution of. the instrument (ΔE/E ≈ 2 × 10⁻⁴) the depth resolution is determined mainly by energy straggling and the combined effect of angular and lateral straggling, and is close to l monolayer near the surface. The mass discrimination of the spectrograph in combination with the energy dispersion of the detector in the focal plane makes possible the background-free detection of light (¹H−¹⁹F) atoms recoiling from a heavier substrate. The design of the total setup is such that channeling and channeling plus blocking experiments can be carried out, so that the position of light (or heavy) atoms on or in monocrystalline samples can be measured. The detector in the focal plane is position-sensitive in two dimensions so that with one setting of the spectrograph an energy range of 2% and an angular distribution of 5° (with a resolution of 0.1°) can be measured simultaneously. The opening angle in the energy-dispersive direction is 0.1°. The whole spectrograph, including the scattering chamber, can be rotated over 120° with respect to the beam line. For this purpose a bellows construction is made between the beam line and the scattering chamber, permitting the rotation while maintaining a vacuum of ≈ 10⁻¹⁰ Torr in the chamber.     

Characterization of extended defects in SiGe alloys formed by high dose Ge implantation into Si

The synthesis of SiGe/Si heterostructures by Ge⁺ ion implantation is reported. 400 keV Ge⁺ ions were implanted at doses ranging from 3 × 10¹⁶ to 10 × 10¹⁶ ions/cm² into (001) Si wafers, followed by Si⁺ amorphisation and low temperature Solid Phase Epitaxial Regrowth (SPER). TEM investigations show that strained alloys can be fabricated if the elastic strain energy (E_el) of the SiGe layer does not exceed a critical value (E′_el) of about 300 mJ/m², which is independent of the implantation energy. Our analysis also suggests that “hairpin” dislocations are formed as strain relieving defects in relaxed structures. A “strain relaxation” model is proposed to explain their formation.     

Range distribution of fluorine in F-implanted LiNbO3

Depth profiles of fluorine in ¹⁹F⁺implanted LiNbO³ have been accurately measured using the ₁₉F(p, γ)¹⁶O resonant nuclear reaction at E_R = 872.1 keV, with Γ = 4.2 keV. A proper convolution calculation method was used to extract the true distribution of fluorine from the experimental excitation yield curves. The experimental range distribution parameters, R_p and ΔR_p, were compared with those obtained by Monte Carlo simulation using a computer code developed recently in this group and with results obtained using the TRIM90 code. It shows that the experimental R_p values agree with the Monte Carlo simulation values very well, while the experimental ΔR_p values are larger than those obtained from the simulations. The simulation with our computer code improves the agreement between the experimental and calculated range straggling, ΔR_p.     

Heavy ion irradiation effects in the rare-earth sesquioxide Dy2O3

Polycrystalline pellets of the rare-earth sesquioxide Dy₂O₃ with cubic C-type rare-earth structure were irradiated with 300 keV Kr²⁺ ions at fluences up to 5 × 10²⁰ Kr/m² at cryogenic temperature. Irradiation-induced microstructural evolution is characterized using grazing incidence X-ray diffraction (GIXRD) and transmission electron microscopy (TEM). In previous work, we found a phase transformation from a cubic, C-type to a monoclinic, B-type (C2/m) rare-earth structure in Dy₂O₃ during Kr²⁺ ion irradiation at a fluence of less than 1 × 10²⁰ Kr/m². In this study, we find that the crystal structure of the top and middle regions of the implanted layer transform to a hexagonal, H-type (P6₃/mmc) rare-earth structure when the irradiation fluence is increased to 5 × 10²⁰ Kr/m²; the bottom of the implanted layer, on the other hand, remains in a monoclinic phase. The irradiation dose dependence of the C-to-B-to-H phase transformation observed in Dy₂O₃ appears to be closely related to the temperature and pressure dependence of the phases observed in the phase diagram. These transformations are also accompanied by a decrease in molecular volume (or density increase) of approximately 9% and 8%, respectively, which is an unusual radiation damage behavior.     

生物样品的同步辐射定量分析

叙述了用同步辐射微探针对生物薄样中向量元素进行定量分析的方法，利用自制的微束标樯测定每个测量点的向量元素面密度并同时根据其在１７－２０ｋｅＶ能区中的Ｃｏｍｐｔｏｎ散射强度确定该测量点的样品质量厚度，成功地实现了元素浓度测量。     

X-ray microprobe – A new facility for cell irradiations in Kraków

A new, multi-purpose X-ray microprobe has been constructed in Kraków. The Hamamatsu L9191 microfocusing X-ray tube is used as a source of radiation. The microprobe is equipped with three dedicated experimental lines serving for the computed microtomography (CMT), for micro-XRF or TXRF measurements (micro-X-ray induced Fluorescence, Total reflexion XRF) and for mammalian cell irradiations. Details of the construction of the experimental line dedicated to irradiations are presented.     

基于反宇宙射线γ谱仪的水样品测量

本文基于本底水平较低的反宇宙射线γ谱仪,对其在水样品测量上的应用进行了探讨。文中使用水标准源对反宇宙射线γ谱仪进行效率刻度,比较不同形状水样品探测效率差异,对采集的某水样品经蒸发浓缩后测量,比较反宇宙γ谱仪与其他γ谱仪测量水样品的探测限。结果γ射线能量E＜130 keV时,反宇宙γ谱仪对马林杯($\phi$17 cm×17 cm)水样品的探测效率低于圆柱体($\phi$7.5 cm×7.0 cm)水样品,而E＞130 keV时,马林杯水样品的探测效率明显大于圆柱体样品。反宇宙γ谱仪测量马林杯水样品的探测限比圆柱体水样品探测限低一个数量级。反宇宙γ谱仪对同一水样品的探测限比常规高纯锗谱仪低一个数量级,该反宇宙γ谱仪直接测量未经前处理马林杯水样品中核素¹⁴⁴Ce、¹³⁷Cs和⁶⁰Co的探测限分别为3.07×10^-2 Bq/L、3.67×10^-3 Bq/L、3.70×10^-3 Bq/L。结论是反宇宙射线γ谱仪可用于低水平放射性水样品测量,其优势在于减少前处理时间,缩短样品测量周期,大大降低探测限,提高测量精确度。     

Accurate quantification resulting from precise beam monitoring and calibration

PIXE investigations in Heidelberg utilize very different target types for which analogous standards are very rarely available. Standardless quantitative measurements are therefore the preferred method. This asks for precise beam monitoring and accurate calibration of the setup for the conversion from X-ray counts to concentrations. It will be shown that our beam monitor enables us to measure beam currents down to 1 pA with a precision of ≈ 0.5%.

The computer code GUPIX which we use to quantify our results offers the possibility to use a calibration function H(E) rather than one constant only. H(E) has been measured, leading to an overall accuracy for quantification of 5% even for trace elements.     

Ion-induced electron emission – monitoring the structure transitions in graphite

The temperature dependence of ion-induced electron emission yield γ under 30 keV Ar⁺ ion impacts at incidence angles θ = 0−80° under dynamically steady-state conditions has been measured for polygranular graphite POCO-AXF-5Q. The fluencies were 10¹⁸–10¹⁹ ion/cm², the temperatures varied from the room temperature (RT) to 400 °C. The RHEED has shown that same diffraction patterns correspond to a high degree of disorder at RT. At high temperature (HT), some patterns have been found similar to those for the initial graphite surfaces. The dependence γ(T) has been found to be non-monotonic and for normal and near normal ion incidence manifests a step-like increase typical for a radiation induced phase transition. At oblique and grazing incidence (θ > 30°), a broad peak was found at T_p = 100 °C. An analysis based on the theory of kinetic ion-induced electron emission connects the behavior of γ(θ,T) to the dependence of both secondary electron path length λ and primary ion ionizing path length R_e on lattice structure that drastically changes due to damage annealing.     

Dissociation of fast HeH ions at glancing angle scattering from a crystal surface

Scattered H⁺ fragments resulting from glancing angle incidence of MeV HeH⁺ ions on the clean (001) surface of a SnTe crystal are distributed on an ellipse in the E-φ plane, where the angle φ is measured in the plane parallel to the surface and E is the energy of the fragment. The kinetic energies released upon dissociation derived from the diameters of the ellipses are smaller than those calculated from the explosion of fully ionized fragments.

Based on a simplified model, we have simulated the dissociative scattering of HeH⁺ ions at the surface, where the dissociation takes place via excitation of HeH⁺ ions and the charges of fragments change along the trajectory. It is concluded from the simulation that the cross section for dissociation in HeH⁺-electron collisions is of the order of 10⁻¹⁶ cm².     

Low energy nitrogen ion doping into GaAs using combined ion-beam and molecular-beam epitaxy method

Low energy nitrogen (N) ions were irradiated during the epitaxial growth of GaAs using combined ion beam and molecular beam epitaxy (CIBMBE) method as a function of N⁺ ion acceleration energy (E_a) and N⁺ ion beam current density (I_N). E_a was varied from 70 to 170 eV I_N from 900 pA/cm² to 75 nA/cm². GaAs growth rate was fixed to 1 μm/h. In 2 K photoluminescence (PL) spectra of the samples with I_N = 3 nA/cm² and E_a = 70–100 eV, two sharp emissions at 1.508 eV (X₁) and 1.495 eV (X₂), which have been attributed to the emissions of excitons bound to isolated N atoms, and another one at 1.443 eV (X₅) were observed. These results show that nitrogen (N) atom in GaAs becomes optically active as an isoelectronic impurity at least in as-grown condition. For N⁺ ion-irradiated samples with rather high I_N, e.g., with I_N = 75 nA/cm² and E_a = 100 eV, a broad emission together with multiple sharp ones were observed after furnace annealing at 750°C which were ascribed to emissions of excitons bound to nitrogen-nitrogen (N---N) pairs.